#------------------------------------------------------------------------------ #$Date: 2022-10-04 17:05:51 +0100 (Tue, 04 Oct 2022) $ #$Revision: 278329 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/01/3500128.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3500128 loop_ _publ_author_name 'Mohanty, Chetna' 'Maris, Thierry' 'Wuest, James D.' _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _publ_section_title ; Aluminium Formate Trihydrate ; _journal_name_full 'Personal communication to COD' _journal_year 2022 _chemical_formula_moiety 'C3 H9 Al O9' _chemical_formula_sum 'C3 H9 Al O9' _chemical_formula_weight 216.08 _chemical_name_common 'Aluminium Formate Trihydrate' _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_Hall '-R 3' _space_group_name_H-M_alt 'R -3 :H' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2022-05-17 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 9.5544(2) _cell_length_b 9.5544(2) _cell_length_c 16.9655(5) _cell_measurement_reflns_used 3594 _cell_measurement_temperature 150 _cell_measurement_theta_max 58.313 _cell_measurement_theta_min 9.608 _cell_volume 1341.23(6) _computing_cell_refinement ; SAINT (2020) V8.40B; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_collection ; APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction ; SAINT (2020) V8.40B; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector 'CMOS Area detector' _diffrn_detector_area_resol_mean 10.42 _diffrn_detector_type 'Bruker CMOS Photon III ' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device 'k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Venture Metaljet' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Helios MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Ga K\a' _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_unetI/netI 0.0256 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 3567 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 58.286 _diffrn_reflns_theta_min 5.174 _diffrn_source 'Metal Jet' _diffrn_source_current 2.85 _diffrn_source_power 0.1986735 _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _diffrn_source_voltage 69.71 _exptl_absorpt_coefficient_mu 1.505 _exptl_absorpt_correction_T_max 0.3076 _exptl_absorpt_correction_T_min 0.2300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0751 before and 0.0384 after correction. The Ratio of minimum to maximum transmission is 0.7477. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.605 _exptl_crystal_description Block _exptl_crystal_F_000 672 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.16 _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Venture diffractometer equipped with a Photon III CMOS Detector, a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode. ; _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _refine_diff_density_max 0.322 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.076 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 52 _refine_ls_number_reflns 620 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.174 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0286 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.3328P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.0660 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 613 _reflns_number_total 620 _reflns_special_details ; _shelx_SHELXL_version_number '2018/3' Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jw24452.cif _cod_data_source_block jw24452 _cod_original_cell_volume 1341.23(7) _cod_original_sg_symbol_H-M 'R -3' _cod_database_code 3500128 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.795 _shelx_estimated_absorpt_t_min 0.733 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-y, x-y, z' 3 '-x+y, -x, z' 4 'x+2/3, y+1/3, z+1/3' 5 '-y+2/3, x-y+1/3, z+1/3' 6 '-x+y+2/3, -x+1/3, z+1/3' 7 'x+1/3, y+2/3, z+2/3' 8 '-y+1/3, x-y+2/3, z+2/3' 9 '-x+y+1/3, -x+2/3, z+2/3' 10 '-x, -y, -z' 11 'y, -x+y, -z' 12 'x-y, x, -z' 13 '-x+2/3, -y+1/3, -z+1/3' 14 'y+2/3, -x+y+1/3, -z+1/3' 15 'x-y+2/3, x+1/3, -z+1/3' 16 '-x+1/3, -y+2/3, -z+2/3' 17 'y+1/3, -x+y+2/3, -z+2/3' 18 'x-y+1/3, x+2/3, -z+2/3' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.666667 0.333333 0.60777(2) 0.01364(18) Uani 1 3 d S T P . . O1 O 0.51333(7) 0.35115(7) 0.67005(4) 0.0180(2) Uani 1 1 d . . . . . O2 O 0.41320(7) 0.44311(7) 0.76041(4) 0.0243(2) Uani 1 1 d . . . . . O3 O 0.50257(7) 0.18123(7) 0.54130(3) 0.0178(2) Uani 1 1 d . . . . . C1 C 0.52576(10) 0.45879(10) 0.71756(5) 0.0192(2) Uani 1 1 d . . . . . H1 H 0.6226(14) 0.5531(14) 0.7190(7) 0.026(3) Uiso 1 1 d . . . . . H3A H 0.4272(17) 0.0877(18) 0.5572(7) 0.031(3) Uiso 1 1 d . . . . . H3B H 0.4586(16) 0.2121(15) 0.5009(9) 0.037(3) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0138(2) 0.0138(2) 0.0133(3) 0.000 0.000 0.00689(10) O1 0.0173(3) 0.0186(3) 0.0184(3) -0.0012(2) 0.0014(2) 0.0092(2) O2 0.0216(3) 0.0211(3) 0.0264(4) -0.0049(2) 0.0061(2) 0.0079(2) O3 0.0171(3) 0.0158(3) 0.0178(3) -0.0004(2) -0.0030(2) 0.0063(2) C1 0.0186(4) 0.0166(4) 0.0205(4) -0.0004(3) 0.0023(3) 0.0075(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.1771 0.1873 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 Al1 O1 91.56(3) 2_655 3_665 O1 Al1 O1 91.56(3) 2_655 . O1 Al1 O1 91.56(3) 3_665 . O1 Al1 O3 177.13(3) 3_665 . O1 Al1 O3 177.13(3) 2_655 3_665 O1 Al1 O3 91.18(2) 3_665 3_665 O1 Al1 O3 91.18(2) 2_655 2_655 O1 Al1 O3 89.25(2) 2_655 . O1 Al1 O3 89.25(2) 3_665 2_655 O1 Al1 O3 89.25(2) . 3_665 O1 Al1 O3 91.18(2) . . O1 Al1 O3 177.13(3) . 2_655 O3 Al1 O3 87.97(3) 2_655 3_665 O3 Al1 O3 87.97(3) . 3_665 O3 Al1 O3 87.97(3) 2_655 . C1 O1 Al1 132.12(5) . . Al1 O3 H3A 123.5(8) . . Al1 O3 H3B 122.1(8) . . H3A O3 H3B 106.5(12) . . O1 C1 H1 117.1(7) . . O2 C1 O1 123.42(8) . . O2 C1 H1 119.4(7) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Al1 O1 1.8818(6) 2_655 Al1 O1 1.8818(6) 3_665 Al1 O1 1.8818(6) . Al1 O3 1.8877(6) 2_655 Al1 O3 1.8877(6) . Al1 O3 1.8877(6) 3_665 O1 C1 1.2647(10) . O2 C1 1.2435(10) . O3 H3A 0.864(15) . O3 H3B 0.926(15) . C1 H1 0.914(12) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C1 H1 O1 0.914(12) 2.668(12) 3.4979(10) 151.5(10) 15_556 yes O3 H3A O2 0.864(15) 1.804(15) 2.6581(9) 169.5(12) 13_556 yes O3 H3B O2 0.926(15) 1.707(15) 2.6310(8) 175.1(13) 9_554 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Al1 O1 C1 O2 -172.26(6) . . . . O1 Al1 O1 C1 110.65(6) 2_655 . . . O1 Al1 O1 C1 19.05(8) 3_665 . . . O3 Al1 O1 C1 -72.11(7) 3_665 . . . O3 Al1 O1 C1 -160.07(7) . . . . _cod_database_fobs_code 3500128